Metals: Experimental and Numerical Simulations of The Solidification Process in Continuous Casting of Slab

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metals

Article
Experimental and Numerical Simulations of the
Solidification Process in Continuous Casting of Slab
Liang Bai, Bo Wang *, Honggang Zhong *, Jie Ni, Qijie Zhai and Jieyu Zhang
State Key Laboratory of Advanced Special Steel, Shanghai University, Shanghai 200072, China;
bailiang410@163.com (L.B.); njpanda@163.com (J.N.); qjzhai@shu.edu.cn (Q.Z.); zjy6162@staff.shu.edu.cn (J.Z.)
* Correspondence: bowang@shu.edu.cn (B.W.); hgzhong@shu.edu.cn (H.Z.); Tel./Fax: +86-021-5633-7547 (B.W.);
Tel.: +86-021-5633-4042 (H.Z.)

Academic Editor: Hugo F. Lopez


Received: 23 December 2015; Accepted: 23 February 2016; Published: 4 March 2016

Abstract: Thermal simulation equipment (TSE) was recently developed to simulate the solidification
process in the industrial continuous casting of slab. The grain growth, solid-liquid interface movement,
and columnar-to-equiaxed transition (CET) in the continuous casting process can be reproduced
using this equipment. The current study is focused on the effects of different cooling rates and
superheat conditions on the grain growth in the solidification process of chromium-saving ferritic
stainless steel (B425). The temperature distribution and microstructure evolution are simulated by a
Cellular Automaton-Finite Element (CAFE) model. The experimental results demonstrate that the
temperature gradient and the grain growth rate of the sample can be effectively controlled by the
equipment. It is observed from optical micrographs of the microstructure that the average equiaxed
grain ratio increases when the superheat temperature decreases. The average equiaxed grain ratio is
approximately 26% and 42% under superheat conditions of 40 ˝ C and 30 ˝ C, respectively, and no
apparent columnar grain generation in the samples occurs under superheat conditions of 10 ˝ C and
20 ˝ C, as the result of a large thermal resistance at the copper-sample interface and low superheat
inside the sample. A lower cooling rate results in a higher equiaxed crystal ratio in the sample.
As the cooling rate decreases, the equiaxed crystal ratio becomes 14%, 23%, and 42%. Comparing the
simulation results with the experimental observations, a reasonable qualitative agreement is achieved
for the chilled layer thickness, grain morphology, and CET in the sample. Thus, the CAFE model in
the current study can accurately predict the grain growth under different superheating and cooling
rate conditions.

Keywords: thermal experimental device; numerical simulation; grain growth; CAFE model

1. Introduction
High temperature, opacity and difficult control are the characteristics of metal solidification
processes. The solidification process is always accompanied by a continuous industrial production.
Therefore, it is difficult to investigate the solidification process for large castings.
An industrial experiment that collects the data directly from the industrial process could directly
reflect the variation in conditions during the production process. It is the most effective guide
for optimizing manufacturing techniques and improving the quality of castings. However, high
temperature and continuous production are the primary difficulties when collecting data. A small
amount of data can be obtained from molten metal. Furthermore, industrial experiment costs are
significant, thus posing considerable challenges and risks for operation. Additionally, under continuous
production conditions, the general experimental methods used in metal solidification investigation,
such as the pouring out method [1], quenching method [2,3], and in-situ observation method [4–8],
cannot be performed.

Metals 2016, 6, 53; doi:10.3390/met6030053 www.mdpi.com/journal/metals


Metals 2016, 6, 53 2 of 12

Over the last several decades, metallurgical technicians have used a considerable amount of labor
and financial resources to obtain technological information during the solidification of a continuous
casting strand. They have designed several modeling experimental types of equipment (such as a
scaled-down continuous caster) to study the continuous casting process in lower solidus temperature
alloys instead of steel [9,10]. These experiments have enabled certain solidification information on the
continuous casting of steel to be obtained; however, due to the difference between the characteristics
of low solidus temperature alloy and steel as well as the different size and manufacturing technique
processes between the experimental equipment and the industrial continuous caster, the process
parameters of industrial continuous casting have been difficult to obtain. Furthermore, the cost of
designing equipment and experimental processes is considerable.
Currently, Zhai [11] has designed a Thermal Simulation Equipment (TSE), which is based on
characteristics similar to that of the heat transfer and grain growth characteristics in a continuous
casting slab. Additionally, the primary heat of the continuous casting of slab is removed in the
thickness and width directions. Furthermore, the heat transfer in the vertical direction is insignificant.
The broad face of the slab is significantly larger than the narrow face. Therefore, the heat transfer
rate of the broad face dominates the heat transfer in the slab. The heat transfer can be considered
to be one-dimensional in most parts of the slab’s cross section. The solidification process of the
continuous casting slab is similar to directional solidification. Nonetheless, the differences between
slab solidification and directional solidification are that the growth speed of the slab thickness is
nonlinear, and the temperature gradient front of the solid-liquid interface is varied. Therefore, by
controlling the temperature and the growth speed, TSE can be used to reproduce grain growth
during the solidification process in the continuous casting of slab to study the grain morphology
variation, solute distribution, columnar-to-equiaxed transition (CET) transformation, and effects of
the technological parameters on the microstructure growth during the solidification process in the
continuous casting of slab.
Compared with industrial and modeling experiments, this thermal simulation method has
more advantages, such as simple operation, easily changeable cooling condition and low cost.
This equipment can be used to optimize the cooling conditions and technology parameters in the
continuous casting process to improve the quality of the product. Furthermore, by combining the
advantages of the numerical and experimental simulations, the results of the experiment can accurately
predict the industrial production process under laboratory conditions.
In this report, TSE was used to study the grain growth under different superheating and cooling
rates in the continuous casting slab. The commercial software ProCAST (2009, ESI, Paris, France)
was used to simulate the grain growth under experimental conditions. The nucleation and growth
parameters of a CA model were validated by the TSE results; thus, the CA model can accurately
describe the grain growth process in the continuous casting of slab.

2. Experimental

2.1. TSE
The schematic diagram of the TSE is illustrated in Figure 1, and the magnification of the furnace
is depicted in Figure 2. The shape and size of the crucible are provided in Figure 3. The vacuum
furnace is divided into a high- (Z1) and low-temperature (Z2) zone (red and light yellow zone in
Figure 2, respectively) by the insulator plate. A hole was drilled into the insulator plate large enough
for the sample to pass through. Before the experiment began, the furnace was moved to location
one (in Figure 1), and the crucible, which is positioned on the water-cooled copper support rod, was
located to the left of the insulator plate, heated to a target temperature at Z1, and held for 10 min;
then, the crucible was placed upside down to complete the pouring process. Liquid metal was poured
into the square from the curved sections. Furthermore, the molten metal contacts the water-cooled
copper sidewall. A chilled layer is rapidly formed on the surface of the sample, and horizontal
Metals 2016, 6, 53 3 of 12

solidification occurs. The equipment keeps the sample stationary, and the driving motor moves the
Metals 2016, 6, 53 3 of 12
furnace backwards
Metals 2016, 6, 53 until solidification is complete. The role of the two-stage heating source 3 of is
12 to
generate a reasonable temperature gradient in the sample, and the insulator plate is located in the
source is to generate a reasonable temperature gradient in the sample, and the insulator plate is
source is to
solid-liquid generateThe
interface. a reasonable
temperaturetemperature gradient
gradient should in thethat
ensure sample, and the insulator
the solid-liquid plate
interface movesis
located in the solid-liquid interface. The temperature gradient should ensure that the solid-liquid
located
with the in the
insulator
Metals 2016, 6, 53solid-liquid
plate at theinterface.
same The temperature
velocity. gradient should ensure that the solid-liquid
3 of 12
interface moves with the insulator plate at the same velocity.
interface moves with the insulator plate at the same velocity.
source is to generate a reasonable temperature gradient in the sample, and the insulator plate is
located in the solid-liquid interface. The temperature gradient should ensure that the solid-liquid
interface moves with the insulator plate at the same velocity.

Figure1.1.Schematic
Schematicof
ofthe
the thermal
thermal simulation
simulationequipment
equipment(TSE).
(TSE).
Figure
Figure 1. Schematic of the thermal simulation equipment (TSE).

Figure 1. Schematic of the thermal simulation equipment (TSE).

Figure 2. Magnification of the furnace.


Figure
Figure2.
Figure 2.2.Magnification of
Magnification of
Magnification the
ofthe furnace.
thefurnace.
furnace.

120mm
120mm
120mm

Figure 3. Size of sample and crucible.


Figure3.3.Size
Figure Size of sample
sampleand
andcrucible.
crucible.

To ensure that the temperature Figurefield and


3. Size of grain
samplegrowth in the sample are consistent with the
and crucible.
To ensure that the temperaturefield
fieldand
and grain
grain growth ininthe
thesample areare
consistent with with
the the
continuous casting slab, the temperature of the heat sources and the
To ensure that the temperature growth movement
sample speed of the furnace
consistent
continuous casting slab, the temperature of the heat sources and the movement speed of the furnace
To to
need
continuousensure thatslab,
becasting
controlledthe bytemperature
thethe fieldofdistribution
temperature
temperature and grainsources
the heat growth
at the andin the
core sample
of the
the arespeed
slab along
movement consistent
withofthe with
thecastingthe
furnace
need to be controlled by the temperature distribution at the core of the slab along with the casting
continuous
direction
need casting
and the
to be controlled slab,
bythe
shell thetemperature
thickness growth
temperature of the
speed heat
of sources
the
distribution slab. and
corethe
However,
at the of movement
the
the speed
temperature
slab along
direction and the shell thickness growth speed of the slab. However, the temperature at the core of
at
withof the
the furnace
thecore of
casting
thethe
need slab
to be and
slab andthetheshell
controlled bythickness
shell growth
growth speed
the temperature
thickness are difficult
difficult
distribution
speed are toobtain
at the
to obtain
core of from
thethe
from theindustrial
slab industrial
along with continuous
the casting
continuous
casting
direction
castingprocess.
and process. Therefore,
the shell thickness
Therefore, these control
growth
these speed
control parameters need
of the slab.
parameters need toto be
However, beobtained
obtained fromthethenumerical
the temperature
from atnumerical
the core of
the slab and the shell thickness growth speed are difficult to obtain from the industrial continuous
casting process. Therefore, these control parameters need to be obtained from the numerical
Metals 2016, 6, 53 4 of 12

direction and the shell thickness growth speed of the slab. However, the temperature at the core of the
slab and the shell thickness growth speed are difficult to obtain from the industrial continuous casting
Metals2016,
Metals 2016,6,6,53
53 4 of12
12
process. Therefore, these control parameters need to be obtained from the numerical simulation 4ofofthe
temperature
simulationofof field
thein the slab. Thefield
temperature numerical model is a two-dimensional slice model, which was slice
first
simulation the temperature field ininthe
theslab.
slab.The
The numericalmodel
numerical modelis isaatwo-dimensional
two-dimensional slice
applied by
model, which Samarasekera
which was was first and Brimacombe
first applied
applied by [12]
by Samarasekerain 1982
Samarasekera and and extensively
and Brimacombe
Brimacombe [12]developed
[12] inin 1982by Thomas
1982 and [13–16].
and extensively
extensively
model,
The parameters
developedby of
byThomas the industrial
Thomas[13–16].
[13–16].The continuous
Theparameters caster
parametersofofthe are listed
theindustrial in Table 1.
industrialcontinuous
continuouscaster
casterarearelisted
listedininTable
Table1.1.
developed
Table 1. Parameters of the continuous caster.
Table1.1.Parameters
Table Parametersofofthe
thecontinuous
continuouscaster.
caster.

Parameter
Parameter
Parameter Value
Value
Value Parameter
Parameter
Parameter Value
Value
Value
Casting
Casting
Casting Speed
Speed
Speed 0.8m/min
0.8
0.8 m/min
m/min Working
Working mold
Workingmold length
moldlength
length 0.8
0.8
0.8m mm
Slab geometry, W × N 200 ×
Slab geometry, W × N 200 × 600
Slab geometry, W ˆ N 200 ˆ 600
600 m Secondary cooling length 13.6 mm
m
m Secondary
Secondarycooling
cooling length
length 13.6
13.6 m
Superheat 20 °C - -
Superheat 20 ˝C - -
Superheat 20 °C - -

The temperature
The
The temperaturecontrol
temperature control
control curves
curves
curves and and
and the movement
thethe movement
movement speed speed
speed
of theofof the
the furnace
furnace furnace are illustrated
are
are illustrated illustrated
in Figuresinin
4
Figures
Figures 4 and 5, respectively.
4 and 5, respectively.
and 5 respectively. The experiments The experiments
The experiments
were conducted were
werewith conducted
conducted with four
with four
four different different superheating
different superheating
superheating temperatures,
temperatures,
˝ C, 20 ˝ C, 3010 ˝ C,°C, 20 °C,
˝ C, 30 °C, and 40 °C, and three different
temperatures, 10 °C, 20 °C, 30 °C, and 40 °C, and three different cooling condition rates.
10 and 40 and three different cooling condition cooling
rates. The condition
temperature rates.
curves The
The
of
temperature
temperature curves of
curves of heat
the high-temperature the high-temperature
the high-temperature
source are depicted heat
heat source
source 4.
in Figure are
areThedepicted
depicted in Figure
in Figure
temperature 4. The
4. The
of the temperature
temperature
low-temperature
of the
of
heatthe low-temperature
low-temperature
source is 110 ˝ C lower heat
heat source
thansource isis 110
the liquidus 110 °C lower
°C lower than
temperature, than the
which the liquidus
canliquidus atemperature,
generatetemperature, which can
which
reasonable temperature can
generate ain
generate
gradient a reasonable
reasonable
the sample. temperature
temperature gradient in
gradient
This phenomenon in the
has the sample.
sample.
been proven This
This phenomenon
phenomenon
several times inhas has been proven
been proven
pre-experiments.
several
several times
times of
The velocity in pre-experiments.
in the
pre-experiments. The velocity
The velocity
furnace is depicted of the
of the
in Figure furnace
furnace
5, where is depicted
is depicted
high, in
mid, andinlow Figure
Figure 5, where
5, where
denote high,
high,
the cooling
mid,and
mid,
rates and
of low
low
the denotethe
denote
slab. thecooling
coolingrates
ratesofofthetheslab.
slab.

Figure4.
Figure
Figure 4.Temperature
4. Temperaturecontrol
Temperature controlcurves
control curvesof
curves ofthe
of thehigh
the hightemperature
high temperatureheat
temperature heatsource.
heat source.(a)
source. (a)Different
(a) Differentsuperheat
Different superheat
superheat
conditions;and
conditions;
conditions; and(b)
and (b)different
(b) differentcooling
different coolingrates.
cooling rates.
rates.

Figure 5. Velocityofofthe
Figure the furnace.(a)
(a) Differentsuperheat
superheat conditions;and
and (b)different
different coolingrates.
rates.
Figure5.5.Velocity
Velocity of thefurnace.
furnace. (a)Different
Different superheatconditions;
conditions; and(b)
(b) different cooling
cooling rates.
2.2.Material
2.2. Material
Thechromium-saving
The chromium-savingferritic
ferriticstainless
stainlesssteel
steelB425
B425was
wasdesigned
designedrecently
recentlyby
byBao
BaoSteel
Steeland
andhas
has
notbeen
not beenbroadly
broadlyapplied
appliedininthe
themarket
marketthus
thusfar.
far.Compared
Comparedwith
with430
430stainless
stainlesssteel,
steel,B425
B425has
hasmore
more
advantages, such as better processing performance and corrosion resistance, lower
advantages, such as better processing performance and corrosion resistance, lower chromium chromium
Metals 2016, 6, 53 5 of 12

2.2. Material
The chromium-saving ferritic stainless steel B425 was designed recently by Bao Steel and has
not been broadly applied in the market thus far. Compared with 430 stainless steel, B425 has more
advantages, such as better processing performance and corrosion resistance, lower chromium content,
and lower cost of production. Furthermore, the solidification process in the continuous casting is
one of the key factors that control the quality of the strand. However, the solidification process of
B425 in continuous casting is not clear. Therefore, this study process could help better understand the
continuous casting solidification process in this new type of steel and guide the optimization process
for the cooling conditions and technical parameters used to improve the slab quality. The chemical
component of B425 was measured by ICP (LEEMAN, Hudson, NH, USA), and set out in Table 2 and
the physical parameters are shown in Table 3.

Table 2. Chemical component of B425 (wt. %).

Elements Cr C N Mn Si P S
Content 14.5 0.025 0.015 0.3 0.3 0.02 0.001

Table 3. Physical properties of B425.

Temperature (K) Fraction Solid (wt. %) Thermal Conductivity (W¨ m´1 ¨ K´1 ) Specific Heat (J¨ g´1 ¨ K´1 )
1783 0.043 32.7 9.02
1781 0.37 33.3 26.8
1778 0.62 33.8 12.9
1776 0.72 33.9 8.87
1773 0.82 34.1 5.64
1771 0.86 34.2 4.40
1768 0.91 34.2 3.22
1766 0.94 34.3 2.70
1763 0.97 34.3 2.16
1761 1.0 34.3 1.89

3. Model Theory
A Cellular Automaton-Finite Element (CAFE) model was used to simulate the grain growth
process of the sample at the same boundary condition as the experimental equipment. The simulation
of nucleation and the growth of grains are built on the macroscopic temperature field. The temperature
field provided vital undercooling data for the micro simulation in the solidification process.
The nucleation model is based on the continuous nucleation theory proposed by Rappaz [17,18].
The CA algorithm, which applies to non-uniform temperature cases, is fully coupled to an
enthalpy-based Finite Element (FE) heat flow calculation. During each time-step, the temperature
in the cell locations is interpolated from those at the FE nodal points to calculate the nucleation and
the growth of grains. The nucleation process is probability density distribution dependent on the
undercooling, and Gaussian distributions have been used to treat the nucleation rate and the nucleation
substrates. The term dn/d∆T is used to describe the grain density increase, dn, which is induced by an
increase in the undercooling, d∆T. Therefore, the total density of the grains, n(∆T), which have been
nucleated at a given undercooling, ∆T, can be described as follows:
ż ∆T
dn
n p∆Tq “ d p∆Tq (1)
0 d p∆Tq
« ff
dn nmax p∆T ´ ∆Tmax q2
“? exp ´ (2)
d p∆Tq 2π∆Tσ 2∆Tσ2
Metals 2016, 6, 53 6 of 12

where, nmax , ∆Tmax , and ∆Tσ are the maximum density of the crystal nucleus, mean undercooling of
the nucleation and standard deviation (the width of the Gaussian curve) at the surface and in the bulk
liquid, respectively.
The KGT model, which is based on a dendrite tip solute balance, was proposed by Kurz, et al. [19].
In the actual simulation process, to accelerate the computation course, the KGT model is fitted, and the
equation can be obtained as follows:

v “ α2 ∆T 2 ` α3 ∆T 3 (3)

where ∆T is the total undercooling of the grain tip; and α2 and α3 are the coefficients of the multinomial
of the grain growth velocity.
« ff
´ρ 1 D2
α2 “ ` (4)
2
2 pm ¨ c0 q p1 ´ kq ¨ Γ ¨ k pm ¨ c 0 q p1 ´ kq ¨ D π2 Γ

D 1
α3 “ ¨ (5)
πΓ pm ¨ c0 q2 p1 ´ kq

where ρ is density of steel, kg/m3 ; m is the liquidus slope, K/wt. %; D is the liquid solute diffusivity,
m2 /s; and k, Γ and c0 is the solute equilibrium partition coefficient, Gibbs-Thompson coefficient and
alloy element initial concentration, respectively. In this report, the pseudo-binary alloy phase diagram
method is applied to address the B425, and this alloy is split into seven Fe-X binary alloy systems,
which are Fe-Cr, Fe-C, Fe-N, Fe-Mn, Fe-Si, Fe-P, and Fe-S. The composition c0 , partition coefficient k,
liquidus slope m, and solute diffusion coefficient Dl of the Fe-X alloys are listed in Table 4.

Table 4. Calculation parameters for α2 and α3 [20–22].

Element c0 /wt. % m/K k Dl /(m2 ¨ s´1 )


Cr 14.5 ´7.4 0.99 1.8 ˆ 10´9
C 0.025 ´58 0.17 2.3 ˆ 10´9
N 0.015 ´4.6 0.78 3.0 ˆ 10´9
Mn 0.3 ´5.0 0.68 7.6 ˆ 10´9
Si 0.3 ´18.7 0.65 8.5 ˆ 10´9
P 0.02 ´48.3 0.13 4.6 ˆ 10´9
S 0.001 ´18.7 0.65 3.5 ˆ 10´9

The calculated value of the liquidus temperature and the solidus temperature of B425 is
Tl = 1783 K and TS = 1758 K, respectively. The Gibbs-Thompson coefficient is Г = 3.2 ˆ 10´7 m¨ K.
The nucleation parameters and growth parameters are listed in Table 5.

Table 5. Nucleation parameters and growth parameters.

Nucleation Parameter ∆T max ∆T σ nmax


Surface nucleation 1.0˝C 2.0 ˝C 4.68 ˆ 109 m´2
Volume nucleation 1.85 ˝ C 1.9 ˝ C 2.82 ˆ 108 m´3
Growth parameter a2 9.403 ˆ 10´6 ms´1 ¨ ˝ C´2
Growth parameter a3 9.480 ˆ 10´6 ms´1 ¨ ˝ C´3
Metals 2016, 6, 53 7 of 12

4. Results and Discussion

4.1. Grain Morphology of the Slab


The industrial continuous casting slab was cut from the center of the wide face, polished using a
grinding machine, and etched. The etching solution, V(HNO3 ):V(HCI):V(HF):V(H2 O) = 2.5:1.5:1:95,
was used to etch the grain boundary, and the metallographic images were observed using a Canon
1500D camera (Canon, Tokyo, Japan). The macrostructure of half of the slab is depicted in Figure 6.
In the figures, the yellow dashed line denotes the CET location. The average length of the columnar
grain 2016,
Metals is approximately
6, 53 69 mm in the slab, and the equiaxial crystal ratio is approximately 31%. 7 of 12
Metals 2016, 6, 53  7 of 12 

Figure
Figure 6.
6. Macrostructure
Macrostructure of
of the
the B425
B425 continuous
continuous casting
casting slab
slab (Provided
  by
(Provided by Bao
Bao Steel).
Steel).
Figure 6. Macrostructure of the B425 continuous casting slab (Provided by Bao Steel). 
4.2. Temperature Distribution in the Furnace
4.2. Temperature Distribution in the Furnace
Figure 2 illustrates the locations of the thermocouples in the furnace, which are marked by the
4.2. Temperature Distribution in the Furnace 
Figure 2 illustrates the locations of the thermocouples in the furnace, which are marked by the
numbers 1 to2  4.
Figure  The temperature
illustrates  distribution
the  locations  in the furnacein 
of  the  thermocouples  was monitored
the monitored by these
furnace,  which  thermocouples.
are thermocouples.
marked  by  the 
numbers 1 to 4. The temperature distribution in the furnace was by these
Thermocouples 1 and
numbers  1  to  4. 1The  2 are used to measure the heat sources at both sides of the heat insulator plate.
Thermocouples andtemperature 
2 are used todistribution 
measure the in heat
the  furnace 
sourceswas  monitored 
at both sides ofby 
thethese 
heat thermocouples. 
insulator plate.
Thermocouples 3 and 4 are used to record the temperature near the heat insulator plate. For example, the
Thermocouples 1 and 2 are used to measure the heat sources at both sides of the heat insulator plate. 
Thermocouples 3 and 4 are used to record the temperature near the heat insulator plate. For example,
experimental temperature distribution under the superheat temperature of 40 °C is depicted in Figure 7.
experimental temperature distribution under the superheat temperature of 40 ˝ C is depicted in
Thermocouples 3 and 4 are used to record the temperature near the heat insulator plate. For example, the 
the
experimental temperature distribution under the superheat temperature of 40 °C is depicted in Figure 7. 
Figure 7. 1600

1550
1600
1500
1550
1450
1500 Liquidus
1400
1450 Liquidus
(℃) (
Temperature

1350
1400
No. 1
Temperature

1300
1350 No. 2
No. 31
No.

1250
1300
)

No. 42
No.
1200
1250 No. 3
HTS CET Solidification end
1150 No. 4
1200
HTS CET Solidification end
1100
1150
0 50 100 150 200 250 300 350 400 450 500 550 600
1100 Time (s)
0 50 100 150 200 250 300 350 400 450 500 550 600
Figure 7. Temperature distribution
Time (s) of the furnace.
Figure 7. Temperature distribution of the furnace. 
Figure 7. Temperature distribution of the furnace.
The HTS is the temperature control curve of the high-temperature heat source. Figure 7
demonstrates that the sample takes
The  HTS  is  the  temperature  control  482 s tocurve 
complete thehigh‐temperature 
of  the  solidification process.
heat  The temperature
source.  Figure  7 
control
The curve
HTS matches
is the well with
temperature the measurement
control curve data
of theof the high-temperature
high-temperature heatheat source
source.
demonstrates  that  the  sample  takes  482  s  to  complete  the  solidification  process.  The  temperature  before7
Figure
482 s. After 482 s, the sample
demonstrates that
control curve matches 
the sample is pulled out of the furnace, and the power for the heat source is shut
takes 482 s to complete the solidification process. The
well with the measurement data of the high‐temperature heat source before 
temperature
off. The
control furnace
curve is cooled
matches by
well natural
with thecooling to roomdata
measurement temperature. Thus, the temperature
of the high-temperature curvebefore
heat source
482 s. After 482 s, the sample is pulled out of the furnace, and the power for the heat source is shut  does
not
482 match between No. 1 and HTS. Furthermore, the low-temperature heat source is accurately
s. After 482 s, the sample is pulled out of the furnace, and the power for the heat
off. The furnace is cooled by natural cooling to room temperature. Thus, the temperature curve does 
source is shut off.
controlled
not  match at 1400 °CNo. 
between  below the HTS. 
1  and  liquidus of 110 °C. the 
Furthermore,  Thislow‐temperature 
result proves that thesource 
heat  temperature of the
is  accurately 
furnace was perfectly controlled through pre-setting during the experimental process.
controlled  at 1400 °C  below the liquidus of 110 °C. This result proves that the temperature of the  The No. 3
curve
furnace indicates a temperature
was  perfectly  change
controlled  near pre‐setting 
through  the left sideduring 
of the heat insulator plate.
the  experimental  The temperature
process.  The  No.  3 
climbed above the liquidus temperature before 262 s. Then, the temperature decreased
curve indicates a temperature change near the left side of the heat insulator plate. The temperature  into the mush
zone, and this temperature curve was parallel with the No.1 curve. This result guarantees a stable
Metals 2016, 6, 53 8 of 12

The furnace is cooled by natural cooling to room temperature. Thus, the temperature curve does not
match between No. 1 and HTS. Furthermore, the low-temperature heat source is accurately controlled
at 1400 ˝ C below the liquidus of 110 ˝ C. This result proves that the temperature of the furnace was
perfectly controlled through pre-setting during the experimental process. The No. 3 curve indicates
a temperature change near the left side of the heat insulator plate. The temperature climbed above
the liquidus
Metals 2016, 6, 53temperature before 262 s. Then, the temperature decreased into the mush zone,8 and of 12
this temperature curve was parallel with the No.1 curve. This result guarantees a stable temperature
Based
gradient in onthethe abovedue
sample control parameters,
to the the solidification
furnace moving backwards. process of the
The CET sampleinwas
location theconducted
sample is
by TSE. Figure
performed from8262depicts
s, andthe
themacrostructure
temperature ofmorphology changes
the solid-liquid under
interface the different
below cooling
the liquidus rates.
causes the
For easy metallographical processing, the samples were cut from the middle (at approximately 5
equiaxed grains to start to nucleate.
cm). After taking photographs, the two images were joined together. The equiaxed grain ratio of the
4.3. Grain Growth
figures was measured using an Image-Pro Plus 6.0 (MEDIA CYBERNETICS, Bethesda, MD, USA).
The grain
Basedmorphology
on the aboveof the slab
control was simulated
parameters, by TSE under
the solidification the same
process of the cooling conditions
sample was and
conducted
superheat
by temperatures.
TSE. Figure 8 depicts The result is illustrated
the macrostructure in Figure 8b.
morphology changes under the different cooling rates.
In Figure
For easy 8b, the length
metallographical of the columnar
processing, grain were
the samples is approximately
cut from the73 mm, and
middle the equiaxial crystal
(at approximately 5 cm).
ratio is
After approximately
taking photographs, 23%. The
the two relative
imageserror
wereofjoined
the columnar
together.grain between grain
The equiaxed the sample
ratio ofand
thethe slab
figures
is 8%, and the size of the grain is slightly larger than the grain size of
was measured using an Image-Pro Plus 6.0 (MEDIA CYBERNETICS, Bethesda, MD, USA). The grainthe slab. However, the
thickness of of
morphology thethechilled layer,
slab was grain morphology,
simulated by TSE under andthe
equiaxial grain generation
same cooling of the
conditions and sample
superheat
agreed well with
temperatures. Thethe industrial
result slab. in Figure 8b.
is illustrated

Figure 8. Macrostructural changes under different cooling conditions. (a) High cooling rate;
Figure 8. Macrostructural changes under different cooling conditions. (a) High cooling rate; (b) middle
(b) middle cooling rate; and (c) low cooling rate.
cooling rate; and (c) low cooling rate.

It can be seen that a chilled layer of approximately 2–3 mm in thickness was generated near the
In Figure 8b, the length of the columnar grain is approximately 73 mm, and the equiaxial crystal
copper surface. Additionally, the thickness of the chilled layer did not change significantly with a
ratio is approximately 23%. The relative error of the columnar grain between the sample and the slab
change in the control parameter. The foremost reason is that the chilled layer is rapidly generated
is 8%, and the size of the grain is slightly larger than the grain size of the slab. However, the thickness
when pouring is complete. A tiny gap was generated between the chilled layer and the copper
of the chilled layer, grain morphology, and equiaxial grain generation of the sample agreed well with
surface due to solidification shrinkage, and the cooling conditions were changed. Therefore, the
the industrial slab.
thickness of the chilled layer is no longer sensitive to the cooling rate, and the thickness will not increase
It can be seen that a chilled layer of approximately 2–3 mm in thickness was generated near the
with an increase in the cooling rate. The CET is gradually brought forward as the cooling rate decreases.
copper surface. Additionally, the thickness of the chilled layer did not change significantly with a
The equiaxed crystal ratio was 14%, 23%, and 42% under high, medium, and low cooling
change in the control parameter. The foremost reason is that the chilled layer is rapidly generated
rates, respectively.
when pouring is complete. A tiny gap was generated between the chilled layer and the copper
To consider the influence of the slag and the Cr/Ni coating at the mold surface on the cooling
surface due to solidification shrinkage, and the cooling conditions were changed. Therefore, the
rate, the interface between the sample and the copper was coated with a thin layer of zirconia. The
thickness of the chilled layer is no longer sensitive to the cooling rate, and the thickness will not
influence of superheat on the grain growth is depicted in Figure 9. The columnar grains only
increase with an increase in the cooling rate. The CET is gradually brought forward as the cooling rate
generated under 30 °C and 40 °C, and the columnar grain increased with an increase in the
decreases. The equiaxed crystal ratio was 14%, 23%, and 42% under high, medium, and low cooling
superheat temperature. The average equiaxed grain rate is approximately 26% and 42% for a
rates, respectively.
superheat temperature of 40 °C and 30 °C, respectively. Additionally, there is no apparent columnar
To consider the influence of the slag and the Cr/Ni coating at the mold surface on the cooling rate,
grain generation in the samples at the superheat temperatures of 10 °C and 20 °C, caused by a large
the interface between the sample and the copper was coated with a thin layer of zirconia. The influence
thermal resistance at the copper-sample interface and a low superheat inside the sample. The
morphology of the grains depends on the G/R ratio, where G and R are the temperature gradient
and the solidification rate, respectively [23]. A low G/R ratio is beneficial for the formation of
equiaxed grains. When the chilled layer is generated, the thermal resistance between the sample
and the water-cooled copper is further increased. As the solidification layer increases, the
Metals 2016, 6, 53 9 of 12

of superheat on the grain growth is depicted in Figure 9. The columnar grains only generated under
30 ˝ C and 40 ˝ C, and the columnar grain increased with an increase in the superheat temperature.
The average equiaxed grain rate is approximately 26% and 42% for a superheat temperature of
40 ˝ C and 30 ˝ C, respectively. Additionally, there is no apparent columnar grain generation in the
samples at the superheat temperatures of 10 ˝ C and 20 ˝ C, caused by a large thermal resistance at
the copper-sample interface and a low superheat inside the sample. The morphology of the grains
depends on the G/R ratio, where G and R are the temperature gradient and the solidification rate,
respectively [23]. A low G/R ratio is beneficial for the formation of equiaxed grains. When the chilled
layer is generated, the thermal resistance between the sample and the water-cooled copper is further
increased. As the solidification layer increases, the temperature gradient decreases from the surface to
the inside of the sample, thus resulting in a low G/R ratio. Thus, the CET transformation is performed
early in the samples under the superheat temperatures of 10 ˝ C and 20 ˝ C. Furthermore, the CET
Metals
occurred 6, 53
2016, at 9 of 12
65 mm and 75 mm under the superheat temperatures of 30 ˝ C and 40 ˝ C, respectively.

˝ C; (b) 30 ˝ C; (c) 20 ˝ C; and (d) 10 ˝ C.


Figure
Figure 9.
9. Influence
Influence of
of superheat
superheat on
on grain
grain growth.
growth. (a)
(a) 40
40 °C; (b) 30 °C; (c) 20 °C; and (d) 10 °C.

Additionally,
Additionally, the the experimental
experimentalresults
resultsindicated
indicated thatthat
thethe columnar
columnar crystal
crystal has ahas a tendency
tendency to grow to
grow
to thetotop thesurface
top surface
of theofsample.
the sample.
This This phenomenon
phenomenon is dueis due
to the to temperature
the temperature difference
difference alongalong
the
the vertical direction of the sample. After pouring, the top surface of the
vertical direction of the sample. After pouring, the top surface of the sample does not contact the sample does not contact the
crucible,
crucible, and and thethe heat
heat transfer
transfer byby convection
convection and and thermal
thermal radiation
radiationisis smaller
smallerthan
thanthatthat inin the
the other
other
area, where the
area, where thesample
sampleand andcrucible
crucible
areare in close
in close contact.
contact. Therefore,
Therefore, the temperature
the temperature at theat topthe top is
is higher
higher
than that than thatbottom
at the at the bottom of the sample.
of the sample. The columnar
The columnar grain the
grain follows follows
heat the
fluxheat flux direction
direction and grows and to
grows to the top surface
the top surface of the sample. of the sample.
Figures
Figures 8b 8b and
and 9c 9c are
are performed
performed at at constant
constant superheat
superheat conditions
conditions and and cooling
cooling rates.
rates. TheThe only
only
difference is that the copper surface is coated with the zirconia layer in Figure 9c. Additionally, G
difference is that the copper surface is coated with the zirconia layer in Figure 9c. Additionally, G isis
the
the driving
driving force force ofof the
the columnar
columnar grain
grain growth.
growth. In InFigure
Figure9c, 9c,G Gisis considerably
considerably lowerlower thanthan that
that ofof the
the
sample
sample without
without coating;
coating; thus,
thus, only
only aa 33 mm
mm long
long columnar
columnar grain grain waswas generated.
generated. TheThe sample
sample without
without
coating
coating generates a large temperature gradient at the front of the chilled layer. R is furtherincreased,
generates a large temperature gradient at the front of the chilled layer. R is further increased,
but
but itit is
is limited
limited by by the
the furnace
furnace movement
movement speed.
speed. Thus,
Thus, the the columnar
columnar grain grain continuously
continuously grows grows until
until
the G/R
the G/R ratio becomes lower than the critical value. A higher intensity at the cooling surface of the
ratio becomes lower than the critical value. A higher intensity at the cooling surface of the
sample
sample generates
generates aa longer
longer columnar
columnar grain
grain inin the
the chilled
chilled layer
layer and
and inside
inside the
the sample.
sample.

4.4.
4.4. Numerical
Numerical Simulation
Simulation Results
Results
The
The solidified structureofofthe
solidified structure thesamples
samples depends
depends critically
critically on on
the the temperature
temperature distribution
distribution and
and fluid
fluid
motionmotion
in thein the molten
molten region.region. In ProCAST,
In ProCAST, the TILTthe TILT was
method method was developed
developed to handle to
thehandle
undesiredthe
undesired
"sticking" "sticking" in thecup
in the pouring pouring
duringcup
tiltduring tilt pouring.
pouring. Here, TILT Here, TILTtois reproduce
is used used to reproduce the tilt
the tilt pouring
pouring
process inprocess in the crucible.
the crucible. Furthermore,
Furthermore, the boundary
the boundary of the
of the sample sample istoidentical
is identical to the
the control control
parameters
parameters of the heat sources and the furnace movement velocity. The simulation result due to the
influence of superheat on the grain growth is depicted in Figure 10.
sample generates a longer columnar grain in the chilled layer and inside the sample.

4.4. Numerical Simulation Results


The solidified structure of the samples depends critically on the temperature distribution and
fluid motion
Metals 2016, 6, 53 in the molten region. In ProCAST, the TILT method was developed to handle 10 ofthe
12
undesired "sticking" in the pouring cup during tilt pouring. Here, TILT is used to reproduce the tilt
pouring process in the crucible. Furthermore, the boundary of the sample is identical to the control
parameters
of of the heat
the heat sources and sources and movement
the furnace the furnacevelocity.
movementThevelocity. Theresult
simulation simulation
due toresult due to the
the influence of
influence of superheat on the grain growth is depicted in Figure 10.
superheat on the grain growth is depicted in Figure 10.

Figure 10.
Figure 10. Numerical
Numerical simulation
simulation result
result of
of the
the grain
grain growth
growth with
with different
different superheat
superheat conditions.
conditions.
(a) 40 °C;
˝ (b) 30 °C;
˝ (c) 20 °C;
˝ and (d) 10
(a) 40 C; (b) 30 C; (c) 20 C; and (d) 10 C. °C.
˝
Metals 2016, 6, 53 10 of 12

There
There are
are three
three distinct
distinct grain zones in
grain zones in the
the samples:
samples: chilled
chilled zone,
zone, columnar
columnar zone,zone, and
and central
central
equiaxed grain zone. The grain morphology transformation is significantly different when the
equiaxed grain zone. The grain morphology transformation is significantly different when the
superheat
superheat temperature
temperature decreases.
decreases. The
TheCET
CETlocation
locationoccurs
occursatat65
65 mmmm andand 7575 mm
mm under
under superheat
superheat
˝ C and 40 ˝ C, respectively. By comparing with the experimental and numerical
conditions of 30 °C and 40 °C, respectively. By comparing with the experimental and numerical
conditions of 30
simulations,
simulations, it
it can
can bebe found
found that
that the
the CAFE
CAFE model
model inin the
the current
current study
study accurately
accurately predicted
predicted the
the grain
grain
morphology
morphology change
change and and CET
CET location
location in
in the
the samples
samples under
under different superheat conditions.
different superheat conditions.
Furthermore, it should be noted that the columnar grains grow obliquely
Furthermore, it should be noted that the columnar grains grow obliquely upwards
upwards to the toptop
to the of
the sample
of the samplein Figure
in Figure 10a,b. TheThe
10a,b. toptop
surface of the
surface sample
of the doesdoes
sample not not
contact the the
contact crucible during
crucible the
during
simulation process;
the simulation thus,thus,
process; the temperature at the at
the temperature topthe
is higher than that
top is higher thanat the
thatbottom
at the of the sample.
bottom of the
The temperature distribution along the vertical direction of the sample is depicted in Figure 11. The
sample. The temperature distribution along the vertical direction of the sample is depicted in Figure 11.
20
Themm, 60 mm,
20 mm, 60 mm, andand 100100
mmmm areare
thethe
distances
distances totothe
thecooling
coolingsurface
surfaceofofthethe sample.
sample. TheThe result
result
indicates that the CAFE model also accurately predicted the columnar grain growth direction.
indicates that the CAFE model also accurately predicted the columnar grain growth direction.

Figure 11. 11.


Figure Numerical simulation
Numerical of theof
simulation temperature distribution
the temperature from the
distribution top the
from to the bottom
top to theofbottom
the sample.
of
the sample.
The numerical simulations of the high, middle, and low cooling conditions were performed
with the same nucleation and growth parameters. The results are presented in Figure 12. It can be
The numerical simulations of the high, middle, and low cooling conditions were performed
observed that the thickness of the chilled layer did not change significantly with a decrease in the
with the same nucleation and growth parameters. The results are presented in Figure 12. It can be
cooling intensity, and the thickness was approximately 2–3 mm. The CET is primarily controlled by
observed that the thickness of the chilled layer did not change significantly with a decrease in the
the ratio of the nucleation rate and the growth rate, and is performed when the nucleation takes the
cooling intensity, and the thickness was approximately 2–3 mm. The CET is primarily controlled by
dominant position. In the samples, the CET gradually moves forward with a decrease in the cooling
the ratio of the nucleation rate and the growth rate, and is performed when the nucleation takes the
rate, and the equiaxed crystal ratio is 13%, 25%, and 40%. Additionally, the columnar crystal tends to
dominant position. In the samples, the CET gradually moves forward with a decrease in the cooling
grow towards the top surface of the sample for the same reason. Compared with the experimental
results, the relative error of the numerical simulations for the high, middle, and low cooling rates is
7.14%, 8.7%, and 4%, respectively.
The numerical simulations of the high, middle, and low cooling conditions were performed
with the same nucleation and growth parameters. The results are presented in Figure 12. It can be
observed that the thickness of the chilled layer did not change significantly with a decrease in the
cooling
Metals intensity,
2016, 6, 53 and the thickness was approximately 2–3 mm. The CET is primarily controlled 11 of by
12
the ratio of the nucleation rate and the growth rate, and is performed when the nucleation takes the
dominant position. In the samples, the CET gradually moves forward with a decrease in the cooling
rate, and the equiaxed crystal ratio is 13%, 25%, and 40%. Additionally,
Additionally, the columnar crystal tends to
grow towards the top top surface of the sample for the samereason.
surface of the sample for the same reason. Compared
Compared with
with the
the experimental
experimental
of the
results, the relative error of the numerical
numerical simulations for the high, middle, and low cooling rates is
respectively.
7.14%, 8.7%, and 4%, respectively.

Figure 12. Grain morphology of the simulation result under different cooling conditions. (a) High
Figure 12. Grain morphology of the simulation result under different cooling conditions. (a) High
cooling rate; (b) middle cooling rate; and (c) low cooling rate.
cooling rate; (b) middle cooling rate; and (c) low cooling rate.

5. Conclusions
5. Conclusions
The grain growth process under different superheat and cooling rate conditions was
The grain growth process under different superheat and cooling rate conditions was investigated
investigated by experimental and numerical simulations. The results indicate that the columnar
by experimental and numerical simulations. The results indicate that the columnar grain is only
generated under superheat conditions of 30 ˝ C and 40 ˝ C, and the columnar grain grows longer as the
superheat temperatures increase. The average length of the columnar grain is approximately 74 mm
and 58 mm at the superheat conditions of 40 ˝ C and 30 ˝ C, respectively. There is no columnar grain
generation in the samples at the superheat conditions of 10 ˝ C and 20 ˝ C, caused by the lower cooling
intensity at the surface of the sample and the temperature gradient inside of the sample. Without the
coating on the copper surface, the CET gradually moves forward, and the equiaxed crystal ratio
increases from 14% to 42% with a decrease in cooling rate.
By comparing the experimental results with the numerical simulations, it can be determined
that the CAFE model in the current study can accurately predict the thickness of the chilled layer,
grain morphology change, and CET location in the samples under different superheat and cooling
rate conditions. The relative error of the numerical simulation for the equiaxed crystal ratio under the
high, middle, and low cooling rates is 7.14%, 8.7%, and 4%, respectively. Thus, the model can provide
guidance for the optimization of TSE.

Acknowledgments: The authors gratefully acknowledge financial support from the National Natural Science
Foundation of China (No. 51227803 and No. 51474143), National Key Technology R & D Program of China
(No. 2012BAE04B02) and Shanghai Economic and Information Commission (No. Hu CXY-2013-1).
Author Contributions: Honggang Zhong and Qijie Zhai conceived and designed the equipment and experiments;
Bo Wang and Jieyu Zhang contributed the numerical simulation; Jie Ni performed the experiments; and Liang Bai
analyzed the data and wrote the report.
Conflicts of Interest: The authors declare no conflict of interest.

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© 2016 by the authors; licensee MDPI, Basel, Switzerland. This article is an open access
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